1、Designation: D 2669 06An American National StandardStandard Test Method forApparent Viscosity of Petroleum Waxes Compounded withAdditives (Hot Melts)1This standard is issued under the fixed designation D 2669; the number immediately following the designation indicates the year oforiginal adoption or
2、, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the determination of the appar-ent viscosity of petrol
3、eum waxes compounded with additives(hot melts). It applies to fluid hot melts having apparentviscosities up to about 20 Pas at temperatures up to 175C(347F).NOTE 1For petroleum waxes and their blends having low apparentviscosities, below about 15 mPas, Test Method D 445, is especiallyapplicable.1.2
4、The values stated in SI units shall be regarded as thestandard. One pascal second (Pas) = 1000 centipoises (cP).One millipascal second (mPas) = 1 centipoise (cgs units).1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility o
5、f the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 445 Test Method for Kinematic Viscosity of Transparentand Opaque Liquids (and Calculation of Dynamic
6、Viscos-ity)E1 Specification for ASTM Liquid-in-Glass ThermometersE 180 Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty Chemicals3. Terminology3.1 Definitions:3.1.1 viscositythe ratio of shear stress to shear rate.Viscosity of a liquid is a
7、measure of the internal friction of theliquid in motion. The unit of dynamic viscosity is the pascalsecond. For a Newtonian liquid, the viscosity is constant at allshear rates. For a non-Newtonian liquid, viscosity will varydepending on shear rate.3.1.2 viscosity, apparentthe viscosity determined by
8、 thismethod, expressed in pascal seconds. Its value may vary withthe spindle and rotational speed selected because many hotmelts are non-Newtonian.4. Summary of Test Method4.1 Approximately 800 g of sample are melted on a hotplate or in an oven. An 800-mL glass beaker which is jacketedwith an electr
9、ic heating mantle is filled with the melted sampleto a level of about 25 mm (1 in.) from its top. The viscometer,with attached spindle and guard, is properly positioned. Stir-ring is begun and continued while the temperature of thesample is brought to slightly above the highest desired testtemperatu
10、re. Heating is discontinued and stirring is maintaineduntil the sample cools to the chosen temperature. At this time,stirring is stopped and the apparent viscosity is determined.Additional determinations are made over a range of tempera-tures as the sample cools. Results of temperature and apparentv
11、iscosity determinations are plotted on semilog paper, andvalues at any particular temperature are determined from thecurve.5. Significance and Use5.1 This test distinguishes between hot melts having differ-ent apparent viscosities. It is believed that apparent viscositydetermined by this procedure i
12、s related to flow performance inapplication machinery operating under conditions of low shearrate. Apparent viscosity as determined by this method may notcorrelate well with end use applications where high shear ratesare encountered.5.2 Materials of the type described in this procedure may bequite n
13、on-Newtonian and as such the apparent viscosity will bea function of shear rate under the conditions of test. Althoughthe viscometer described in this test generally operates underconditions of relatively low shear rate, differences in shear1This test method is under the jurisdiction of ASTM Committ
14、ee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.10 on Properties of Petroleum Wax.Current edition approved July 1, 2006. Published August 2006. Originallyapproved in 1967. Last previous edition approved in 1999 as D 266987(1999),which was withdrawn in N
15、ovember 2004 and reinstated in July 2006.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM Inte
16、rnational, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.effect can exist depending upon the spindle and rotationalspeed conditions selected for the test program. Maximumcorrelation between laboratories, therefore, depends upon test-ing under conditions of equiv
17、alent shear.6. Apparatus6.1 ViscometerBrookfield Synchro-Lectric Viscometer,Models LVF or LVT with numbers 1, 2, 3, and 4 stainless steelspindles and V-shaped stand with leveling screws.6.2 Glass Beaker, 800-mL Griffin standard form.6.3 Glass Heating Mantle, for 800-mL beaker.6.4 Autotransformer, va
18、riable.36.5 Thermometers,ASTM Precision Thermometer 88C hav-ing a range from 10 to 200C or Thermometer 88F having arange from 50 to 392F as prescribed in Specification E1aresuitable.6.6 Laboratory Stirrer Motor, variable speed.6.7 Propeller and Shaft, stainless steel 51 mm (2 in.) indiameter, three
19、blades to fit 7.9 by 475-mm (516 by 18-in.)stainless steel shaft.6.8 Hot Plate, with continuously adjustable temperaturecontrol.6.9 Laboratory Jack, scissors-type.6.10 Ring Stands and Clamps, for mounting stirrer andthermometer.6.11 Semilog Graph Paper, two cycles.7. Procedure7.1 Selection of Spindl
20、eFrom the estimated viscosity ofthe sample and Table A1.1, select a spindle size and speedcombination that preferably will produce readings within therange recommended by the manufacturer. Attach the spindle tothe viscometer, with guard attached and mount the instrumenton its stand.NOTE 2Care must b
21、e taken while storing and handling the spindle. Itshould be protected from dust, corrosive deposits, and mechanical abuse.Avoid touching the calibrated section of the spindle with the hands.Thoroughly clean it and the guard after each use.7.2 Preparation of SampleIn a suitable container, meltapproxi
22、mately 800 g representative of the sample to be testedon a hot plate or in an oven. Bring the temperature of thesample to 120 to 150C (250 to 300F) and stir to ensurehomogeneity, taking care not to whip air into the meltedsample. Fill the 800-ml test beaker with the melted sample toa level about 25
23、mm (1 in.) from the top. Place the filled beakerinto the heating mantle which is supported by the laboratoryjack in its lowered position. Connect the heating mantle to theautotransformer which, in turn, is connected to the proper acsupply. Connect the viscometer to its proper ac supply. Positionthe
24、viscometer with spindle and guard attached, the stirrer, andthermometer as shown in Figs. A1.1 and A1.2. Mount thethermometer so that the center of its bulb is in the samehorizontal plane as the center of the test section of the spindle,and spaced approximately the same distance as the guard fromthe
25、 spindle, about 13 mm (12 in.). Position the stirring propellerabout midway between the bottom of the guard and the bottomof the beaker. Position the complete assembly so that the testportion of the spindle is spaced approximately 19 mm (34 in.)from the side of the beaker when the beaker containing
26、thesample is in the operating position. Raise the beaker containingthe sample by means of the laboratory jack so that the spindleis covered to about 6 mm (14 in.) below its immersion mark.Adjust the stirrer speed to give maximum agitation of the testsample without permitting vortex or air bubble inc
27、lusion.Apply heat to the sample by adjusting the autotransformer, andraise its temperature to about 5C (10F) above the highest testtemperature. Maintain stirring throughout the heating cycle,being careful to prevent air entrainment in the sample.NOTE 3As the temperature of the sample increases, its
28、liquid levelwill approach the immersion mark on the spindle. Be careful to preventthe sample level from rising above the immersion mark on the spindle.Final immersion adjustment shall be made just before viscometer readingsare determined.7.3 Viscosity DeterminationWhen the temperature of thesample r
29、eaches 5C (10F) above the highest test temperature,shut off the autotransformer, start the viscometer motor, andcontinue stirring. The temperature of the sample will begin tolower, and when it becomes 0.5C (1F) above the intendedtest temperature, stop the stirrer, but continue the spindlerotation. W
30、ait 5 s, and readjust the viscometer to the immersionmark on the spindle. Allow the spindle to make three completeadditional rotations. Engage the pointer clutch, and stop theviscometer motor when the pointer is in view. Record the dialreading. Restart the viscometer motor, release the clutch, maket
31、hree additional spindle revolutions, engage the clutch, andstop the viscometer motor when the pointer is in view. Recordthe second dial reading, and repeat the above operation toobtain a total of three readings which should be completedwithin a period of about 1 min. During this time the tempera-tur
32、e of the sample should fall no lower than 0.5C (1F) belowthe intended test temperature. Record the three test readingsand the test temperature. Immediately after the final reading,start the stirrer motor and viscometer with the clutch engaged.Permit the temperature of the sample to drop about 15C(25
33、F), and repeat the same procedure at a lower temperature.Continue this sequence to produce dial readings at four or moredifferent temperatures, each spaced approximately 15C (25F)lower than the preceding test temperature.NOTE 4The range of test temperatures shall include all temperaturesat which app
34、arent viscosity values are desired. Minor vertical adjustmentsof the spindle may be required to maintain its proper immersion as thevolume of the sample decreases with lower temperatures.8. Calculation8.1 Determine the averages of the three scale readings madefor each test temperature. Calculate the
35、 apparent viscosities, inpascal seconds or millipascal seconds, by multiplying theaverage viscometer scale reading for each test temperature bythe factor indicated in Table A1.1 for the spindle and speedcombination used.3The sole source of supply of the apparatus known to the committee at this timei
36、s the Variac Type W5 MT, IET Labs, Inc. 534 Main Street, Westbury, NY 11590.If you are aware of alternative suppliers, please provide this information to ASTMInternational Headquarters. Your comments will receive careful consideration at ameeting of the responsible technical committee,1which you may
37、 attend.D26690628.2 Plot the apparent viscosity values obtained on the logscale, and the corresponding test temperatures on the linearscale of appropriate semilog paper. From the plot, determinethe apparent viscosity of the sample at any temperature withinthe range of the test temperatures.9. Report
38、9.1 Report the apparent viscosity at a given temperaturewith the spindle number and speed used to obtain the data as:Apparent viscosity, 325 mPas at 120C (1)No. 2 spindle, 30 rpm!10. Precision and Bias10.1 The composition of a hot melt influences the precisionto be expected when testing different ty
39、pes of samples. Thefollowing data should be used to judge the acceptability ofresults (95 % probability) for four different types of hot meltsaccording to the concept of precision as given in PracticeE 180.10.2 Duplicate results should be considered suspect if theydiffer by more than the following a
40、mounts for each of the fourtypes listed: below:10.2.1 High-Viscosity Sample, M1-65-20:58 weight % of a 68C (155F) melting point wax.42 weight % of an ethylene-vinyl acetate copolymer con-taining 27 to 29 % vinyl acetate and having a melt index offrom 12 to 18.Viscosity,mPasTemperature, Repeatability
41、,mPasReproducibility,mPasC (F)11 200 121 (250) 1900 24007500 134 (275) 1200 17005100 149 (300) 660 150010.2.2 Medium-Viscosity Sample, MI-65-21:72 weight % of a 61C (142F) melting point wax.28 weight % of the same copolymer used in sample MI-65-20.Viscosity,mPasTemperature, Repeatability,mPasReprodu
42、cibility,mPasC (F)1200 121 (250) 81 240840 134 (275) 63 150610 149 (300) 47 12010.2.3 Low-Viscosity Sample, MI-65-22:96.3 weight % of a 77C (170F) melting point microcrys-talline wax.2.7 weight % of butyl rubber.Viscosity,mPasTemperature, Repeatability,mPasReproducibility,mPasC (F)68 121 (250) 15 32
43、52 134 (275) 11 2941 149 (300) 7.9 2210.2.4 Low-Viscosity Sample, MI-65-23:80 weight % of a 68C (154F) melting point wax.20 weight % of a 5000 molecular weight polyethylenehaving a melting point from 107 to 111C (224 to 232F), aspecific gravity of 0.92 and a typical viscosity at 140C of 4Pas.Viscosi
44、ty,mPasTemperature, Repeatability,mPasReproducibility,mPasC (F)25 121 (250) 1.9 4.420 134 (275) 1.2 4.016 149 (300) 1.5 3.810.3 BiasThe procedure in this test method has no biasbecause the value of apparent viscosity can be defined only interms of a test method.11. Keywords11.1 apparent viscosity; h
45、ot melts; petroleum waxes; waxesANNEX(Mandatory Information)A1. SELECTION OF SPINDLE AND PREPARATION OF SAMPLEA1.1 Table A1.1 lists spindle size and spindle speed, Fig.A1.1 and Fig. A1.2 present a top and side view of the testapparatus.TABLE A1.1 Viscometer Spindle Number-Speed-Maximum Viscosity Rel
46、ationshipSpindle NumberSpindle Speed, rpm60 30 12 6125101. Multiplication factor viscosity, max, mPas 100520010500251000502. Multiplication factor viscosity, max, mPas 50020100040250010050002003. Multiplication factor viscosity, max, mPas 2000100400020010 00050020 00010004. Multiplication factor vis
47、cosity, max, mPas 10 000 20 000 50 000 100 000D2669063FIG. A1.1 Viscosity Test Apparatus, Side ViewFIG. A1.2 Viscosity Test Apparatus, Top ViewD2669064ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Use
48、rs of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every
49、 five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is co
